CN112851878A - High-solid-content polymer polyol and preparation method thereof - Google Patents
High-solid-content polymer polyol and preparation method thereof Download PDFInfo
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- 229920005862 polyol Polymers 0.000 title claims abstract description 189
- 150000003077 polyols Chemical class 0.000 title claims abstract description 189
- 229920000642 polymer Polymers 0.000 title claims abstract description 155
- 238000002360 preparation method Methods 0.000 title abstract description 37
- 238000004917 polyol method Methods 0.000 title description 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 154
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 78
- 229920000570 polyether Polymers 0.000 claims abstract description 78
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 74
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims abstract description 35
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims abstract description 34
- MVELOSYXCOVILT-UHFFFAOYSA-N (4-hydroxy-2-methylpentan-2-yl) 7,7-dimethyloctaneperoxoate Chemical compound CC(O)CC(C)(C)OOC(=O)CCCCCC(C)(C)C MVELOSYXCOVILT-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims description 38
- 238000006116 polymerization reaction Methods 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 47
- 239000000243 solution Substances 0.000 description 28
- 238000009833 condensation Methods 0.000 description 23
- 239000000178 monomer Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- 150000002148 esters Chemical class 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 150000003254 radicals Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 125000003636 chemical group Chemical group 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/006—Removal of residual monomers by chemical reaction, e.g. scavenging
Abstract
The invention discloses a high-solid content polymer polyol, which belongs to the technical field of polyether polyol and is prepared from the following components in parts by weight: 1-5 parts of hydroxyethyl methacrylate; 33-55 parts of polyether polyol; 25-35 parts of styrene; 10-20 parts of acrylonitrile; 0.1-0.5 part of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate; 0.1-1 part of isopropanol; 1-10 parts of polyether derivative. The preparation method comprises the following steps: mixing the materials related to the formula at normal temperature and normal pressure to prepare a reaction solution; then continuously injecting the reaction liquid into a reaction kettle, controlling the reaction temperature at 115-125 ℃, controlling the reaction pressure at 0.3-0.5 MPa, and keeping the reaction materials for 2 hours to prepare polymer polyol; finally, the prepared polymer polyol is subjected to molecular removal and oil-free vortex vacuum treatment, and vacuum demoistening is carried out for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa. The invention has the beneficial effects that: the obtained high solid content polymer polyol has the characteristics of good stability, low viscosity and low VOC.
Description
Technical Field
The invention relates to the technical field of polyether polyol, and particularly relates to high-solid-content polymer polyol and a preparation method thereof.
Background
Zhong Chong Min et al uses polypropylene glycol-400, maleic anhydride and propylene oxide as raw materials to prepare a macromonomer, and then uses polyether polyol 330 as basic polyether to synthesize macromonomer polyether derivatives, thereby solving the problem of POP stability. The macromolecular monomer polyether derivative is subjected to a grafting reaction with styrene and acrylonitrile under the action of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate to synthesize polymer polyol, and the morphology of the surface of a dispersed particle is measured by a polarizing microscope. The results show that: with the increase of the amount of the macromonomer, the stability gradually becomes better. When the using amount of the macromonomer is 10% -15% of that of the polyether derivative, a large amount of paste-like agglomerates are formed on the wall of the flask, and when the using amount is 30%, the stability of the system is greatly improved, the number of agglomerated particles is small, and the generated particles are uniform.
Shu Zhongfeng et al use polyether polyol, TDI and hydroxyethyl acrylate as raw materials to synthesize a macromonomer DP6000, use the macromonomer as a polyether derivative precursor to participate in the synthesis reaction of POP, and explore the influence of the macromonomer dosage on the POP performance. The results show that: with the increase of the amount of the macromonomer, the POP viscosity is reduced and then increased, and the particle size is continuously reduced. When the addition mass fraction is less than 1%, the POP system is not stable enough, and the phenomenon of adhesion and caking exists; with the increase of the using amount of the polyether derivative, when the mass fraction reaches 2.5%, the system is stable, and the viscosity is 5000 mPas. When the mass fraction reaches 3.5%, the viscosity of the system rises quickly. Therefore, when the mass fraction of the polyether derivative is 2.5-3.5%, the system stability is the best.
Zhang et al improved the problems of high product viscosity, large production odor and high monomer content when the existing high solid content polymer polyol adopts an intermittent production process, prepared the high solid content polymer polyol by adopting a continuous production process to replace the intermittent production process, and synthesized the high solid content polymer polyol by adopting novel polyether derivative TBF and novel liquid peroxide peroxyneodecanoic acid-1, 1-dimethyl-3-hydroxybutyl ester POP 2. The novel production process reduces the viscosity of polymer polyol, reduces the odor and VOC of the product, has good adaptability to a foaming formula system when being applied to polyurethane foaming, and greatly improves the overall performance of the product.
The Shandong Longhua New materials Co., Ltd discloses in a patent a process for preparing polymer polyols using a continuous process. Polyether polyol and olefinic unsaturated monomer are firstly synthesized into macromolecular monomer, then the macromolecular monomer, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, isopropanol, styrene and acrylonitrile are jointly used for preparing a stabilizer system, and finally the macromolecular monomer, the styrene, the acrylonitrile and the polyether polyol are polymerized in the presence of the isopropanol and the 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate to prepare polymer polyol. The solid content of the polymer polyol prepared by the method is high, the self-made macromolecular monomer is adopted to control the particle size of the obtained polymer polyol, the viscosity of a system is obviously reduced, and the VOC is also controlled and reduced to be below 100 PPm.
Zhao Bao Cheng et al developed a novel chain transfer polyether derivative BDF-5A. The viscosity of the product at 25 ℃ is less than 1000 mPa.s, and isopropanol does not need to be added when the product is used for synthesizing POP, so that the product not only can be used in the Huahualu production process, but also the production cost can be saved, and the VOC emission can be greatly reduced. The POP produced with the BDF-5A polyether derivative has higher non-volatile content, lower viscosity and smaller polymer particle size. And polyurethane foam made with such POP has good strength and elongation.
The patent of China petrochemical group company introduces a process for continuously preparing POP by using 2-3 serially connected reaction kettles. The method is characterized in that basic polyether polyol, styrene, acrylonitrile, isopropanol, a solvent, a polyether derivative and free radicals are initiated and then continuously introduced into a first reaction kettle, when kettle materials overflow into a pipeline of a second reaction kettle, free radical peroxyneodecanoate-1, 1-dimethyl-3-hydroxybutyl ester is introduced into the pipeline, the free radical peroxyneodecanoate-1, 1-dimethyl-3-hydroxybutyl ester enters the second reaction kettle together with auxiliary materials to be continuously polymerized, and a crude POP product obtained by overflowing from the last reaction kettle is sent to a post-treatment process. According to the method, the free radical peroxyneodecanoic acid-1, 1-dimethyl-3-hydroxybutyl ester is added in sections, so that the conversion rates of styrene and acrylonitrile are greatly improved, the load of a single removing process is reduced, and the VOC in the POP is greatly reduced.
The Wanhua chemical group introduced an improved POP VOC removal process in the patent. It comprises the following steps: 1. removing most of styrene, acrylonitrile and isopropanol in the POP through vacuum evaporation by a thin film evaporator or a supergravity evaporator at the temperature of 110-140 ℃ and under the condition of 2-10 kPa to obtain a POP intermediate; 2. adding a finishing agent (toluene) with the mass fraction of 5-11.6% into the intermediate, and stirring for 0.5-3.0 h at the temperature of 60-100 ℃; 3. adding an inert solvent (i-propylcyclohexane) with the mass of 1.1-1.8 times of that of the mixed solution, and stripping and removing the finishing agent and the solvent at the temperature of 110-140 ℃ and under the condition of 2-10 kPa to obtain a final POP product. The total mass fraction of residual monomers and isopropanol in the POP obtained by the method is less than 20 multiplied by 10 < -6 >, the surface of POP polymer particles is smooth, and the viscosity is reduced by 300-1000 mPa & s compared with that before treatment.
Zhushu et al developed a novel isopropyl alcohol for POP. The compound is a similar compound with the average molecular weight of 100-180, and research results of the compound used for synthesizing POP show that compared with the traditional POP, the POP prepared by using the novel isopropanol has higher content of non-volatile matters and lower viscosity. Since the novel isopropyl alcohol has a relatively high boiling point, it is not emitted as VOC.
Wanhua chemical group, Inc. introduced in the patent a method for preparing POP with low odor and high weatherability by using azocarboxylic ester peroxyneodecanoic acid-1, 1-dimethyl-3-hydroxybutyl ester and titanate catalyst to compose a composite radical peroxyneodecanoic acid-1, 1-dimethyl-3-hydroxybutyl ester. The titanate is preferably propyl titanate and/or butyl titanate, which can be used as a catalyst to enable the polyether polyol to perform transesterification reaction with the azocarboxylic ester and the decomposition coupling product thereof, thereby further reducing the odor and VOC of the POP. In addition, the titanate compound can be converted into TiO2 under the hydrolysis condition, can generate photoelectric effect under the illumination condition, generates high-activity free radicals, further endows the POP with the effects of sterilization and oxidation resistance, and can also enhance the weather resistance of the POP.
As far as the research is concerned, the polymer polyol has poor stability, viscosity and VOC content when it has high solid content.
Disclosure of Invention
Aiming at the problems of poor stability, high viscosity, high VOC content and the like of high-solid-content polymer polyol in the prior art, the invention provides high-solid-content polymer polyol which is prepared from the following components in parts by weight:
preferably, the composition is prepared from the following components in parts by weight:
preferably, the composition is prepared from the following components in parts by weight:
preferably, the solid content of the polymer polyol is 42-49%; the viscosity is 4500-7000 mPa.s/25 ℃; styrene is less than or equal to 5 ppm.
Preferably, the amount of the hydroxyethyl methacrylate is 3-5% of the total amount of the styrene and the acrylonitrile.
The invention also provides a preparation method of the high-solid-content polymer polyol, which comprises the following steps:
the method comprises the following steps: mixing hydroxyethyl methacrylate, polyether polyol, styrene, acrylonitrile, polyether derivatives, isopropanol and 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demoistening for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required high-solid-content polymer polyol.
Hydroxyethyl methacrylate with a hydroxyl and unsaturated bond structure and a polyether derivative are compounded and used as one of reaction monomers to react with styrene and acrylonitrile, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a reactive hydroxyl function, and the problem of stability of the polymer polyol at high solid content is solved. The high-purity 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate is used as an initiator, all decomposers are nontoxic oxygen-containing volatile gases, the purity is high, and compared with azobisisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low. Meanwhile, a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the preparation method with the recovery rate of the residual monomer of 5 per mill is environment-friendly, the VOC is low, and the polymer polyol has high solid content polymer polyol with good stability, low viscosity and low VOC.
Has the advantages that:
the technical scheme of the invention has the following beneficial effects:
(1) hydroxyethyl methacrylate with a hydroxyl and unsaturated bond structure and a polyether derivative are compounded and used as one of reaction monomers to react with styrene and acrylonitrile, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a reactive hydroxyl function, the problem of stability of the polymer polyol with high solid content is solved, and the solid content of the prepared polymer polyol is 42-49%; the viscosity is 4500-7000 mPa.s/25 ℃; styrene is less than or equal to 5 ppm.
(2) The high-purity 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate is used as an initiator, all decomposers are nontoxic oxygen-containing volatile gases, the purity is high, and compared with azobisisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low.
(3) The preparation method has the advantages that a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the recovery ratio of the residual monomer is 5 per mill, the preparation method is environment-friendly, the VOC is low, and the polymer polyol has high solid content polymer polyol with good stability, low viscosity and low VOC.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention will be described in detail and completely with reference to the examples of the present invention, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, provided in the examples, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the embodiment, hydroxyethyl methacrylate and polyether derivative with hydroxyl and unsaturated bond structures are compounded and used as one of reaction monomers to react with styrene and acrylonitrile, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a reactive hydroxyl function, and the problem of stability of the polymer polyol at high solid content is solved. The specific technical scheme is as follows:
the high-solid-content polymer polyol is prepared from the following components in parts by weight:
the composition is prepared from the following components in parts by weight:
the composition is prepared from the following components in parts by weight:
as a preferred embodiment, the solid content of the polymer polyol is 42-49%; the viscosity is 4500-7000 mPa.s/25 ℃; styrene is less than or equal to 5 ppm.
In a preferred embodiment, the amount of hydroxyethyl methacrylate is 3 to 5% of the total amount of styrene and acrylonitrile.
The embodiment also provides a preparation method of the high-solid-content polymer polyol, which comprises the following steps:
the method comprises the following steps: mixing hydroxyethyl methacrylate, polyether polyol, styrene, acrylonitrile, polyether derivatives, isopropanol and 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demoistening for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required high-solid-content polymer polyol.
Hydroxyethyl methacrylate with a hydroxyl and unsaturated bond structure and a polyether derivative are compounded and used as one of reaction monomers to react with styrene and acrylonitrile, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a reactive hydroxyl function, and the problem of stability of the polymer polyol at high solid content is solved. The high-purity 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate is used as an initiator, all decomposers are nontoxic oxygen-containing volatile gases, the purity is high, and compared with azobisisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low. Meanwhile, a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the preparation method with the recovery rate of the residual monomer of 5 per mill is environment-friendly, the VOC is low, and the polymer polyol has high solid content polymer polyol with good stability, low viscosity and low VOC.
The beneficial effects of the powder and the annular inductor obtained by the technical solution of the present embodiment are further described below by several sets of examples and comparative examples.
The first embodiment is as follows:
the preparation method of the polymer polyol in this example includes the following steps:
the method comprises the following steps: mixing 2 parts by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Example two:
the preparation method of the polymer polyol in this example includes the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example one:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 0.5 part by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example two:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 6 parts by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example three:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 25 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example four:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 70 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example five:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 20 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example six:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 45 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example seven:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 7 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example eight:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 27 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example nine:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example ten:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.05 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example eleven:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.8 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example twelve:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example thirteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.05 part by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example fourteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 1.3 parts by weight of isopropanol and 2.5 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example fifteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate and 0.58 part by weight of isopropanol at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example sixteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 0.5 part by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example seventeen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.7 parts by weight of hydroxyethyl methacrylate, 33 parts by weight of polyether polyol, 28 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 12 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example eighteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 3 parts by weight of hydroxyethyl methacrylate, 45 parts by weight of polyether polyol, 30 parts by weight of styrene, 17 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 12 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example nineteen:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 1.2 parts by weight of hydroxyethyl methacrylate, 50 parts by weight of polyether polyol, 28 parts by weight of styrene, 18 parts by weight of acrylonitrile, 0.25 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.58 part by weight of isopropanol and 12 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example twenty:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 2 parts by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: and continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, wherein the reaction temperature is controlled to be 115-125 ℃, the reaction pressure is controlled to be 0.3-0.5 MPa, and the residence time of the reaction materials is 2 hours, so as to prepare the polymer polyol.
Comparative example twenty one:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 2 parts by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 110 ℃, the reaction pressure at 0.1MPa and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
Comparative example twenty-two:
the preparation method of the polymer polyol in the comparative example comprises the following steps:
the method comprises the following steps: mixing 2 parts by weight of hydroxyethyl methacrylate, 40 parts by weight of polyether polyol, 34 parts by weight of styrene, 20 parts by weight of acrylonitrile, 0.3 part by weight of 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate, 0.7 part by weight of isopropanol and 3 parts by weight of polyether derivative at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum de-condensation for 4 hours at the temperature of 170 ℃ and under the pressure of-0.15 MPa, and removing small molecular substances to finally prepare the required polymer polyol.
The polymer polyols prepared in the two groups of examples and the twenty-two groups of comparative examples are subjected to data tests on solid content, viscosity, styrene content and the like, and specific data are as follows:
TABLE 1 sets of examples and comparative examples Polymer polyol test data
As can be seen from Table 1, the polymer polyol obtained by the formulation and the process can maintain a viscosity within a certain range while maintaining a suitable solid content, and has styrene content of less than or equal to 5ppm and a low moisture content. The high solid content polymer polyol has the characteristics of better stability, low viscosity and low VOC.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The high-solid-content polymer polyol is characterized by being prepared from the following components in parts by weight:
2. a high solids polymer polyol as claimed in claim 1, prepared from the following components in parts by weight:
3. a high solids polymer polyol as claimed in claim 1, prepared from the following components in parts by weight:
4. a high solids polymer polyol as claimed in claim 1, wherein the polymer polyol has a solids content of 42 to 49%; the viscosity is 4500-7000 mPa.s/25 ℃; styrene is less than or equal to 5 PPm.
5. A high solids polymer polyol as claimed in claim 1, wherein the amount of hydroxyethyl methacrylate is 3-5% of the total amount of styrene and acrylonitrile.
6. A process for preparing a high solids polymer polyol as claimed in any one of claims 1 to 5, comprising the steps of:
the method comprises the following steps: mixing hydroxyethyl methacrylate, polyether polyol, styrene, acrylonitrile, polyether derivatives, isopropanol and 1, 1-dimethyl-3-hydroxybutyl peroxyneodecanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature at 115-125 ℃, the reaction pressure at 0.3-0.5 MPa, and the residence time of the reaction materials at 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 4 hours at the temperature of 140-160 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required high-solid-content polymer polyol.
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Application publication date: 20210528 |
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